A new sol-gel system using acetoin was developed and employed for the fabrication of PZT powders and films with compositions near the morphotropic phase boundary Pb(Zr0.52Ti0.48)O-3. Acetoin was used as chelating agent to replace the highly toxic methoxyethanol used in previous formulations. This route simplified the chemical processing of PZT-based solutions. Powders were completely crystallized by about 450 degrees C and contained the ferroelectric perovskite single phase. The firing temperature and time were to be the most important variables. Metallic lead formed only when excess Pb was incorporated. The precursor and the heat-treated powders have been characterized by using thermal analysis and X-ray diffractometry (XRD) studies. The average particle size, as measured from X-ray line broadening, was similar to 35 nm.